CN113953525A - Preparation method of nanowire silver film for packaging and interconnecting large-size power semiconductor integrated circuit - Google Patents
Preparation method of nanowire silver film for packaging and interconnecting large-size power semiconductor integrated circuit Download PDFInfo
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- CN113953525A CN113953525A CN202111207769.7A CN202111207769A CN113953525A CN 113953525 A CN113953525 A CN 113953525A CN 202111207769 A CN202111207769 A CN 202111207769A CN 113953525 A CN113953525 A CN 113953525A
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- 238000003825 pressing Methods 0.000 claims abstract description 10
- 238000000967 suction filtration Methods 0.000 claims abstract description 9
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
Abstract
The invention discloses a preparation method of a nanowire silver film for packaging and interconnecting large-size power semiconductor integrated circuits, which comprises the steps of diluting and purifying a silver nanowire mother solution, and obtaining the nanowire silver film after filter pressing or suction filtration and drying. The preparation method provided by the invention has the advantages of simple process, low cost and controllable film thickness. The nanowire silver film prepared by the invention has the characteristics of easy film formation, less organic matter and other impurities, higher structural strength, low-temperature sintering realization, convenient and efficient use, high reliability, high thermal conductivity, high conductivity, low porosity and the like of the film layer after hot-pressing sintering.
Description
Technical Field
The invention relates to the technical field of electronic packaging, in particular to a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit.
Background
At present, the interconnection of chip substrates of high-power semiconductor integrated circuits is mostly realized by adopting nano silver films. The nano silver film on the market is mostly prepared from nano silver particles, the film forming property of particle raw materials is poor, organic matters such as a film forming agent and a dispersing agent are generally required to be added, and the film is prepared by adopting the processes such as a tape casting method and a coating method. Although the content of nano silver particles in the silver film is up to 99%, the content of organic matters is still higher, namely about 1%. The silver film prepared by the nano silver particles has the defects of process adaptability, service performance and the like in the packaging interconnection process, and firstly, the silver film transfer process is complex and needs special equipment to implement: the nano-particle silver film has low strength and cannot be directly transferred to the surface of a chip or a substrate, the chip is usually attached to the silver film by using customized equipment, the preliminary bonding between the chip and the silver film is realized by presintering, and then the chip is transferred to the substrate to be subjected to hot-pressing sintering so as to obtain the packaging interconnection between the chip and the substrate. And the thermal conductivity and the connection strength of the packaging interconnection layer are lower. Residual organic matters in the silver film sintering layer are difficult to remove in the packaging interconnection hot-pressing sintering process, and the nano silver particles are almost in point contact, so that more interfaces and pores can be formed on the sintering layer. The microstructure characteristics of the silver film sintering layer are not beneficial to improving the performances such as the thermal conductivity, the electric conductivity and the connection strength of the film layer, and the requirements of high thermal conductivity, electric conductivity, high connection strength and other service performances of high-power device packaging and interconnection are difficult to meet.
Disclosure of Invention
The invention provides a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit, which is used for overcoming the defects of process adaptability, use performance and the like in the prior art.
In order to achieve the above purpose, the invention provides a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit, which comprises the following steps:
s1: diluting and purifying the silver nanowire mother solution to obtain a silver nanowire dispersion solution;
s2: carrying out filter pressing or suction filtration on the silver nanowire dispersion liquid to obtain a wet nanowire silver film;
s3: and drying the wet nanowire silver film to obtain the nanowire silver film.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the nano-particle silver film which needs large-scale equipment such as a casting machine, a coating machine and the like, the preparation method of the nano-wire silver film for packaging and interconnecting the large-size power semiconductor integrated circuits provided by the invention only needs filter pressing or suction filtration, and has the advantages of simple equipment and process, stable performance and batch production.
2. According to the preparation method provided by the invention, the organic matter content in the nanowire silver film is lower (less than 0.3%), the residual carbon of the hot-pressed sintering layer of the nanowire silver film is less, the porosity is lower, the thermal conductivity is high, the electrical conductivity is better, and the connection strength is higher.
3. The chip is not matched with the substrate in the process of sintering due to expansion with heat and contraction with cold, so that stress is easily generated, and the existence of the stress is unfavorable for the weather resistance, the reliability and the like of the device. According to the preparation method provided by the invention, the silver film sintering layer has a porous structure, and the porous silver film structure can buffer stress generated during sintering, so that the reliability of the device is improved. Namely, the microstructure of the nanowire silver film prepared by the invention can reduce the thermomechanical stress caused by the thermal mismatch between the chip and the substrate and improve the reliability of the device in the service process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a scanning electron microscope image of silver nanowires in example 1;
FIG. 2 is a scanning electron microscope photograph of a silver film of nanowires in example 1;
fig. 3 is a physical diagram of the nanowire silver film in example 1.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific mention.
The invention provides a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit, which comprises the following steps:
s1: diluting and purifying the silver nanowire mother solution to obtain a silver nanowire dispersion solution;
s2: carrying out filter pressing or suction filtration on the silver nanowire dispersion liquid to obtain a wet nanowire silver film;
s3: and drying the wet nanowire silver film to obtain the nanowire silver film.
Preferably, in step S1, the dilution is specifically:
and diluting the silver nanowire mother liquor by 2-20 times by adopting a diluent. The dilution is to dissolve the organic matter coated on the surface of the silver nanowire into diluents such as water, ethanol and the like, so as to achieve the purpose of purification.
Preferably, the diluent is ethanol, deionized water or other alcohol low-boiling organic solvents. The silver nanowire prepared by the alcohol heating method is coated with a layer of organic matter which can be dissolved in alcohol or dissolved in water. The film is then pressed and dried at low temperature, so that water or low boiling point alcohol solvent is needed.
Preferably, in step S1, the purification specifically includes:
and (3) placing the diluted silver nanowire mother liquor into a water bath kettle at the temperature of 30-60 ℃ and stirring for 0.5-2 h to obtain the silver nanowire dispersion liquid. The purification principle is that the organic matter on the surface layer of the silver nanowire can be dissolved in water or alcohol, and the organic matter coating layer on the surface layer of the silver nanowire can be thinned until the organic matter coating layer is not formed by adding a sufficient amount of diluent.
The purpose of purification is that the organic matter coating layer on the surface of the silver nanowire can influence the electric conduction and heat conduction performance of the packaged device, and the silver nanowire needs to be cleaned to meet the use requirement of a high-power device.
Preferably, in the step S2, the pressure of the filter pressing or suction filtration is 0.5-2 MPa. The purpose of filter pressing or suction filtration is to extract silver nanowires in the mother liquor, solid silver nanowires are left on the filter pressing membrane or the filter pumping membrane, and other liquid substances are filtered by the filter pressing membrane or the filter pumping membrane, so that the purpose of solid-liquid separation is achieved. The silver nanowires have small size which is as low as 20nm, and the mother liquor is difficult to pass through a filter membrane or a suction filter membrane when the pressure of filter pressing or suction filtration is small, so that the aim of solid-liquid separation cannot be achieved. When the pressure is too high, the filter membrane or the suction filter membrane made of organic materials is broken.
Preferably, in step S3, the drying is specifically:
and transferring the wet nanowire silver film onto a plastic film, and drying for 1-3 h at 40-80 ℃ to obtain the nanowire silver film. The reason for transferring to the plastic film is that the nano silver film has a small thickness, generally 30 to 70 μm, and a low strength, and needs to be placed on a support for transportation and use.
Preferably, the plastic film is one of polyethylene, polypropylene, polyvinyl chloride, polystyrene and polyethylene terephthalate. Different plastic materials have different surface tensions and different adsorption forces on the nanowire wet film. The tension is too large, and the silver film is easy to transfer; the tension is too small, the adsorption force between the silver film and the plastic film is larger, and water or alcohol solvent between the films is not easy to volatilize during drying.
Preferably, the thickness of the nanowire silver film is 30-70 mu m, and the content of organic matters and other impurities is less than 0.3%.
Preferably, the diameter of the silver nanowires in the silver nanowire mother liquor is 20-200 nm, and the length of the silver nanowires is 5-50 μm.
The preparation method of the nanowire silver film for packaging and interconnecting the high-power semiconductor integrated circuit, provided by the invention, adopts the silver nanowires to prepare the silver film, and the silver nanowires have small diameter and low melting point effect and can be sintered by hot pressing at low temperature. The sintered body (film) has melting point close to that of bulk silver (961 ℃), and can be used at high temperature, and has good heat and electric conductivity and high shear strength.
The preparation method provided by the invention adopts the silver nanowires to prepare the film, the length of the silver nanowires is 5-50 mu m, the silver nanowires are alternately and interactively lapped, the film is easier to form, the structural integrity of the silver film is good, and the thickness of the silver film is thinner, uniform and controllable.
Preferably, the silver nanowire mother solution is prepared by a conventional alcohol heating method; the mass fraction of the silver nanowires in the silver nanowire mother liquor is 0.5-0.6%. Example 1
The embodiment provides a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit, which comprises the following steps:
s1: the silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, wherein silver nanowires in the silver nanowire mother liquor are shown in figure 1, the diameter of the silver nanowires is 100-150 nm, and the length of the silver nanowires is 25-35 mu m.
Putting 0.5L of silver nanowire mother liquor into a beaker, taking normal-temperature deionized water according to the proportion of 1:10 of the silver nanowire mother liquor, and adding the deionized water into the beaker to dilute the silver nanowire mother liquor;
and (3) placing the beaker in a water bath at the temperature of 30 ℃ and stirring for 2 hours at the stirring speed of 500r/min to obtain the silver nanowire dispersion liquid.
S2: and (3) carrying out pressure filtration on the silver nanowire dispersion liquid under the pressure of 0.5MPa to obtain a wet nanowire silver film. The pressure filtration membrane of this example is a hydrophilic polytetrafluoroethylene microporous membrane with a pore size of 0.45 μm. The support of the wet nanowire silver film in this example was a polyethylene terephthalate film.
S3: and (3) drying the wet nanowire silver film in a vacuum furnace at the temperature of 40 ℃ for 2h to obtain the nanowire silver film, wherein the silver nanowires in the nanowire silver film are mutually overlapped together as shown in figures 2 and 3, and the nanowire silver film has good integrity.
The thickness of the nanowire silver film prepared by the embodiment is 45 μm, and the content of organic matters is 0.22%.
Example 2
The embodiment provides a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit, which comprises the following steps:
s1: the silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the diameter of a silver nanowire in the silver nanowire mother liquor is 50-80 nm, and the length of the silver nanowire in the silver nanowire mother liquor is 20-33 mu m.
Putting 0.7L of silver nanowire mother liquor into a beaker, taking normal-temperature deionized water according to the proportion of 1:16 of the silver nanowire mother liquor, and adding the deionized water into the beaker to dilute the silver nanowire mother liquor;
and (3) placing the beaker in a water bath at 50 ℃ and stirring for 0.5h at the stirring speed of 500r/min to obtain the silver nanowire dispersion liquid.
S2: and (3) carrying out pressure filtration on the silver nanowire dispersion liquid under the pressure of 0.5MPa to obtain a wet nanowire silver film. The pressure filtration membrane of this example is a hydrophilic polytetrafluoroethylene microporous membrane with a pore size of 1 μm. The carrier of the wet nanowire silver film in the embodiment is a polypropylene plastic film.
S3: and (3) drying the wet nanowire silver film for 1h in a vacuum furnace at the temperature of 50 ℃ to obtain the nanowire silver film, wherein the nanowire silver film has good structural integrity, and silver nanowires in the nanowire silver film are alternately overlapped.
The silver film thickness of the silver nanowire prepared by the embodiment is 57 μm, and the organic matter content is 0.24%.
Example 3
The embodiment provides a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit, which comprises the following steps:
s1: the silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the diameter of silver nanowires in the silver nanowire mother liquor is 160-200 nm, and the length of the silver nanowires is 5-18 mu m.
Putting 1L of silver nanowire mother liquor into a beaker, taking ethanol according to the proportion of 1:2 of the silver nanowire mother liquor, and adding the ethanol into the beaker to dilute the silver nanowire mother liquor;
and (3) placing the beaker in a water bath at 60 ℃ and stirring for 0.7h at the stirring speed of 500r/min to obtain the silver nanowire dispersion liquid.
S2: and (3) carrying out pressure filtration on the silver nanowire dispersion liquid under the pressure of 1MPa to obtain a wet nanowire silver film. The pressure filtration membrane of this example is a hydrophilic polytetrafluoroethylene microporous membrane with a pore size of 1 μm. The support of the wet nanowire silver film in this embodiment is a polystyrene film.
S3: and (3) drying the wet nanowire silver film for 1.2h in a vacuum furnace at the temperature of 80 ℃ to obtain the nanowire silver film, wherein the nanowire silver film has good structural integrity, and silver nanowires in the nanowire silver film are alternately lapped in an alternating manner.
The silver film thickness of the silver nanowire prepared by the embodiment is 30 μm, and the organic matter content is 0.21%.
Example 4
The embodiment provides a preparation method of a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit, which comprises the following steps:
s1: the silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the diameter of a silver nanowire in the silver nanowire mother liquor is 20-45 nm, and the length of the silver nanowire in the silver nanowire mother liquor is 35-50 mu m.
Putting 0.2L of silver nanowire mother liquor into a beaker, taking ethanol according to the proportion of 1:20 of the silver nanowire mother liquor, and adding the ethanol into the beaker to dilute the silver nanowire mother liquor;
and (3) placing the beaker in a water bath at 40 ℃ and stirring for 2h at the stirring speed of 500r/min to obtain the silver nanowire dispersion liquid.
S2: and (3) carrying out pressure filtration on the silver nanowire dispersion liquid under the pressure of 2MPa to obtain a wet nanowire silver film. The pressure filtration membrane of this example is a hydrophilic polytetrafluoroethylene microporous membrane with a pore size of 0.5 μm. The support of the wet nanowire silver film in this embodiment is a polystyrene film.
S3: and (3) drying the wet nanowire silver film for 2.1h in a vacuum furnace at the temperature of 70 ℃ to obtain the nanowire silver film, wherein the nanowire silver film has good structural integrity, and silver nanowires in the nanowire silver film are alternately lapped in an alternating manner.
The silver film thickness of the silver nanowire prepared by the embodiment is 70 μm, and the organic matter content is 0.23%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method for preparing a nanowire silver film for packaging and interconnecting a large-size power semiconductor integrated circuit is characterized by comprising the following steps:
s1: diluting and purifying the silver nanowire mother solution to obtain a silver nanowire dispersion solution;
s2: carrying out filter pressing or suction filtration on the silver nanowire dispersion liquid to obtain a wet nanowire silver film;
s3: and drying the wet nanowire silver film to obtain the nanowire silver film.
2. The method according to claim 1, wherein in step S1, the dilution is specifically:
and diluting the silver nanowire mother liquor by 2-20 times by adopting a diluent.
3. The method of claim 2, wherein the diluent is ethanol, deionized water or other alcohol low boiling point organic solvent.
4. The method according to any one of claims 1 to 3, wherein in step S1, the purification is specifically:
and (3) placing the diluted silver nanowire mother liquor into a water bath kettle at the temperature of 30-60 ℃ and stirring for 0.5-2 h to obtain the silver nanowire dispersion liquid.
5. The method according to claim 1, wherein in step S2, the pressure of the pressure filtration or suction filtration is 0.5 to 2 MPa.
6. The method according to claim 1, wherein in step S3, the drying is specifically:
and transferring the wet nanowire silver film onto a plastic film, and drying for 1-3 h at 40-80 ℃ to obtain the nanowire silver film.
7. The method of claim 6, wherein the plastic film is one of polyethylene, polypropylene, polyvinyl chloride, polystyrene, and polyethylene terephthalate.
8. The preparation method according to claim 1, wherein the thickness of the nanowire silver film is 30-70 μm, and the content of impurities such as organic matters is less than 0.3%.
9. The method according to claim 1, wherein the silver nanowires in the silver nanowire mother liquor have a diameter of 20 to 200nm and a length of 5 to 50 μm.
10. The preparation method according to claim 1, wherein the silver nanowire mother liquor is prepared by a conventional alcohol heating method; the mass fraction of the silver nanowires in the silver nanowire mother liquor is 0.5-0.6%.
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| CN202111207769.7A CN113953525B (en) | 2021-10-18 | 2021-10-18 | Preparation method of nanowire silver film for packaging and interconnecting large-size power semiconductor integrated circuit |
| PCT/CN2022/095116 WO2023065666A1 (en) | 2021-10-18 | 2022-05-26 | Preparation method for nanowire silver film for packaging and interconnection of large-size power semiconductor integrated circuit |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023065666A1 (en) * | 2021-10-18 | 2023-04-27 | 国防科技大学 | Preparation method for nanowire silver film for packaging and interconnection of large-size power semiconductor integrated circuit |
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